Search Results (161)

L. ferrooxidans and their metabolic products have been explored as viable flotation reagents of pyrite and chalcopyrite for froth flotation. Scanning electron microscopy (SEM), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, time-of-flight secondary ion mass spectrometry (ToF-SIMS) and captive bubble contact angle measurements have been used to examine the surface physicochemical properties of pyrite upon exposure to L. ferrooxidans grown in HH medium at pH 1.8. C K-edge NEXAFS spectra, collected using scanning transmission X-ray microscopy (STXM), indicate hydrophilic lipids, fatty acids, and biopolymers are formed at the mineral–bacterium interface within hours of exposure. The Fe L-edge NEXAFS show oxidation of the mineral surface from Fe (II) sulfide to Fe (III) oxyhydroxides. The leaching of the iron species at the pyrite surface is accelerated in the presence of L. ferrooxidans and extracellular polymeric substances (EPS) as compared to HH medium controls, as shown by ToF-SIMS. The surface chemical changes induced by the interaction with L. ferrooxidans show a significant decrease in surface hydrophobicity within the first 2 h of exposure. The implications of these findings are the potential use of EPS, produced during early attachment of L. ferrooxidans, as a depressant for bioflotation or to enhance bioleaching. Full article

Composite materials based on low-density polyethylene (LDPE) embedded with iron-manganese nanoparticles with compositions Fe_0.9Mn_0.1 and Fe_0.8Mn_0.2 were prepared and investigated. The newly created composites were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray absorption near-edge structure (XANES), extended X-ray absorption fine structure (EXAFS), and Mössbauer spectroscopy. The composition, electronic, and atomic structure of the nanoparticles were established. The study confirms that the nanoparticles possess a ‘core-shell’ structure, the nature of which depends on the manganese content. The nanoparticles of Fe_0.8Mn_0.2 in LDPE exhibit a three-layered structure: a metallic α-Fe core is coated with an intermediate oxidized layer structurally close to Fe₂O₃, while the outermost shell consists of manganese oxide (Mn₂O₃). In contrast, nanoparticles with lower Mn content Fe_0.9Mn_0.1 show a predominantly fully oxidized structure. This structural evolution is consistent with thermodynamic principles, where manganese, having a higher oxide formation enthalpy, migrates to the surface. The core–shell architecture is promising for applications requiring stable magnetic components or tailored catalytic interfaces within a polymer matrix. Full article

A recently discovered turquoise deposit in the Fangshankou area of Dunhuang, Gansu Province, has been relatively understudied compared to turquoise from other sources due to its short mining history. Currently, no relevant research literature on this deposit has been identified. Therefore, a systematic mineralogical and spectroscopic study of Dunhuang turquoise samples was conducted using conventional gemological testing methods, combined with techniques such as X-ray powder diffraction (XRD), electron probe microanalysis (EPMA), Fourier transform infrared spectroscopy (FTIR), laser Raman spectroscopy, ultraviolet-visible spectroscopy (UV-Vis), and X-ray fluorescence (XRF) mapping. The test results indicate that the turquoise samples from this area have a density ranging from 2.40 to 2.77 g/cm³ and a refractive index between 1.59 and 1.65. The samples generally exhibit a cryptocrystalline structure, with some displaying spherulitic radial and radial fibrous structures. The texture is relatively dense and hard, with particle diameters less than 10 μm. Chemically, the turquoise samples from this region are characterized by high Fe and Si content and relatively low Cu content. Samples contain, in addition to the turquoise mineral, other minerals such as quartz, goethite and alunite, etc. The oxide content ranges are as follows: w(P₂O₅) between 23.83% and 33.66%, w(Al₂O₃) between 26.47% and 33.36%, w(CuO) between 5.26% and 7.91%, w(FeO) between 2.46% and 4.11%, and w(SiO₂) between 0.97% and 10.75%. In the infrared absorption spectra of Dunhuang turquoise, the bands at 3510 cm⁻¹ and 3464 cm⁻¹ are attributed to ν(OH)⁻ stretching vibrations, while the bands near 3308 cm⁻¹ and 3098 cm⁻¹ are assigned to ν(M-H₂O) stretching vibrations. The infrared absorption bands near 1110 cm⁻¹ and 1058 cm⁻¹ are due to v[PO₄]³⁻ stretching vibrations, and the bands near 651 cm⁻¹, 575 cm⁻¹, and 485 cm⁻¹ are attributed to δ[PO₄]³⁻ bending vibrations. A clear correlation exists between the Raman spectral features and the infrared spectra of this turquoise. The hue and chroma of the turquoise from this area are primarily influenced by the mass fractions of Fe³⁺, Cu²⁺, and Fe²⁺, as well as their bonding modes with water molecules. The ultraviolet-visible spectra are attributed to O²⁻–Fe³⁺ charge transfer, the ⁶A₁–⁴E_g + ⁴A₁ transition of Fe³⁺ ions (D⁵ configuration) in hydrated iron ions [Fe(H₂O)₆]³⁺, and the spin-allowed ²E_g–²T_2g transition of Cu²⁺ ions in hydrated copper ions [Cu(H₂O)₄]²⁺. Associated minerals include goethite, alunite, jarosite, and quartz. Fine-grained quartz often exists as secondary micron-sized independent mineral phases, which have a certain impact on the quality of the turquoise. Full article

Double perovskites are represented by the formula A₂BB’O₆ and AA’BB’O₆. These materials have been synthesized using the solid-state reaction, sol–gel, Pechini, and hydrothermal methods. X-ray fluorescence, X-ray diffraction, magnetic measurements, transmission electron microscopy, X-ray photoelectron spectroscopy, temperature-programmed reduction, synchrotron X-ray diffraction, neutron powder diffraction, extended X-ray absorption fine structure, and Raman spectroscopy have been used for the characterization of double perovskites. X-ray diffraction, synchrotron X-ray diffraction, and neutron powder diffraction coupled with the Rietveld method determine the crystal structure of a sample. These materials present various properties and applications. The present review aims (i) to report a process to determine the symmetry, apparent size, and apparent strain using the Rietveld method; (ii) show how experimental characterization techniques complement each other in the investigation of double perovskites; (iii) describe how the synthesis method can help in the uncovering of double perovskites with improved properties; and (iv) exemplify some of the main applications of double perovskites. Full article

High-efficiency diesel and lean-burn engines produce lower exhaust temperatures, which can delay the activation of after-treatment catalysts such as Diesel Oxidation Catalysts (DOCs). This study explores ion beam sputtering as a post-synthesis strategy to enhance the low-temperature activity of commercial Pt/CeO₂–ZrO₂ catalysts. Low-energy ions (0.5–1.5 keV) were applied with controlled variations in treatment number, beam current, and exposure time to selectively generate oxygen vacancies and improve Pt dispersion. Structural and chemical effects were characterized using X-ray diffraction (XRD), BET surface area measurements, X-ray photoelectron spectroscopy (XPS) and extended X-ray absorption fine structure (EXAFS). Catalytic performance was evaluated through CO and C₃H₆ oxidation under conditions mimicking lean-burn engine exhaust. Increasing the number of ion treatments progressively lowered light-off temperatures, correlating with enhanced Pt–Ce³⁺ interactions and improved surface reducibility. Variations in beam current and exposure time further modulated these surface effects, confirming the tunable nature of the approach. The results demonstrate that ion beam sputtering selectively modifies the catalyst surface without altering the bulk structure, directly linking atomic-scale modifications to improved low-temperature activity. This strategy offers a promising route to overcome delayed light-off issues in modern high-efficiency engines, providing a precise, controllable method to optimize emission control catalysts. Full article

The increasing demand for sustainable construction materials has prompted the recycling of construction and demolition waste in concrete manufacturing. This study investigates the feasibility of utilizing porcelain and brick waste as partial substitutes for natural sand in concrete with the objective of improving sustainability and preserving mechanical and durability characteristics. The experimental program was conducted in three consecutive phases. During the initial phase, natural sand was partially substituted with porcelain waste powder (PWP) and brick waste powder (BWP) in proportions of 25%, 50%, and 75% of the weight of the fine aggregate. During the second phase, polypropylene fibers were mixed at a dosage of 0.5% by volume fraction to enhance tensile and flexural properties. During the third phase, zinc oxide nanoparticles (ZnO-NPs) were utilized as a partial substitute for cement at concentrations of 0.5% and 1% to improve microstructure and strength progression. Concrete samples were tested at curing durations of 7, 28, and 91 days. The assessed qualities encompassed workability, density, water absorption, porosity, compressive strength, flexural strength, and splitting tensile strength. Microstructural characterization was conducted utilizing X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS). The findings indicated that porcelain waste powder markedly surpassed brick waste powder in all mechanical and durability-related characteristics, particularly at 25% and 50% sand replacement ratios. The integration of polypropylene fibers enhanced fracture resistance and ductility. Moreover, the incorporation of zinc oxide nanoparticles improved hydration, optimized the pore structure, and resulted in significant enhancements in compressive and tensile strength throughout prolonged curing durations. The best results were obtained with a mix of 50% porcelain sand aggregate, 1% zinc oxide nanoparticles as cement replacement, and 0.5% polypropylene fibers, for which the improvements in compressive strength, flexural strength, and splitting tensile strength were 39.5%, 46.2%, and 60%, respectively, at 28 days. The results confirm the feasibility of using porcelain and brick waste as sand replacements in concrete, as well as polypropylene fiber-reinforced concrete and polypropylene fiber-reinforced concrete mixed with zinc oxide nanoparticles as a sustainable option for construction purposes. Full article

X-ray absorption spectroscopy (XAS) and X-ray emission spectroscopy (XES) are analytical techniques enabling precise analysis of the electronic structure and local atomic environment in chemical compounds and materials. Their application spans materials science, chemistry, biology, and environmental sciences, supporting studies on catalytic mechanisms, redox processes, and metal speciation. A key advantage of both techniques is element selectivity, allowing the analysis of specific elements without matrix interference. Their high sensitivity to chemical state and coordination enables determination of oxidation states, electronic configuration, and local geometry. These methods are applicable to solids, liquids, and gases without special sample preparation. Modern XAS and XES studies are typically performed using synchrotron radiation, which provides an intense, monochromatic X-ray source and allows advanced in situ and operando experiments. Sub-techniques such as XANES (X-ray absorption near-edge structure), EXAFS (Extended X-ray Absorption Fine Structure), and RIXS (resonant inelastic X-ray scattering) offer enhanced insights into oxidation states, local structure, and electronic excitations. Despite their broad scientific use, applications in pharmaceutical research remain limited. Nevertheless, recent studies highlight their potential in analyzing crystalline active pharmaceutical ingredients (APIs), drug–biomolecule interactions, and differences in drug activity. This review introduces the fundamental aspects of XAS and XES, with an emphasis on practical considerations for pharmaceutical applications, including experimental design and basic spectral interpretation. Full article

We present a systematic study of the fundamental optical properties of indium selenide (InSe) single crystals over a temperature range of 17 K to 300 K. The high structural quality of the β-polytype crystals was confirmed through X-ray diffraction, Raman spectroscopy, and high-resolution transmission electron microscopy, demonstrating excellent crystallinity and a nearly stoichiometric In:Se ratio. The temperature-dependent absorption and photoluminescence (PL) spectra are characterized by a prominent free exciton (FX) resonance. At 17 K, the photoluminescence spectrum exhibits a distinct fine-structure splitting of the Wannier–Mott exciton, yielding a triplet state at 1.333 eV and a singlet state at 1.336 eV. Additionally, a biexciton (XX) is localized at an energy of 1.322 eV as confirmed by the nonlinear dependence of intensity on excitation power density. At low temperatures, the absorption spectrum exhibits the free exciton ground state (n = 1) at 1.338 eV together with the first excited state (n = 2) at 1.350 eV. We systematically tracked and analyzed the temperature evolution of these quasiparticle energies. These findings enhance our understanding of the intrinsic many-body interactions in high-quality InSe, providing essential parameters for advancing its applications in innovative optoelectronic and quantum light-emitting devices. Full article

Carbon nanotubes (CNTs) have remarkable mechanical, electrical, and thermal properties, making them highly attractive as foundational elements for advanced materials. However, translating their nanoscale potential into macroscale reliability and longevity requires a holistic design approach that integrates precise architectural control with robust damage mitigation strategies. This review presents a synergistic perspective on enhancing the durability of CNT-based systems by critically examining the interplay between molecular assembly, self-repair mechanisms, and the advanced characterization techniques required for their validation. We first establish how foundational architectural control—achieved through strategies like chemical functionalization, field-directed alignment, and dispersion—governs the ultimate performance of CNT materials. A significant focus is placed on advanced functionalization, such as fluorination, and its verification using high-powered spectroscopic tools, including X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. Subsequently, this manuscript delves into the mechanisms of self-repair, systematically analyzing both the intrinsic capacity of the carbon lattice to heal atomic-level defects and the extrinsic strategies that incorporate engineered healing agents into composites. This discussion is uniquely supplemented by an exploration of the experimental techniques, such as electron energy loss spectroscopy (EELS) and Auger electron spectroscopy (AES), that provide crucial evidence for irradiation-induced healing dynamics. Finally, we argue that a “characterization gap” has limited the field’s progress and highlight the critical role of techniques like in situ Raman spectroscopy for quantitatively monitoring healing efficiency at the molecular level. By identifying current challenges and future research frontiers, this review underscores that the creation of truly durable materials depends on an integrated understanding of how to build, repair, and precisely measure CNT-based systems. Full article

Complex oxides with the general formula Gd₂(Ti_1−xZr_x)₂O₇ are promising candidates for radioactive waste immobilization due to their capacity to withstand radiation by dissipating part of the free energy driving defect creation and phase transitions. In this study, samples with varying zirconium content (xZr = 0.00, 0.15, 0.25, 0.375, 0.56, 0.75, 0.85, 1.00) were synthesized via the sol–gel method and thermally treated at 500 °C to obtain nanosized powders mimicking the defective structure of irradiated materials. Synchrotron-based techniques were employed to investigate their structural properties: High-Resolution X-ray Powder Diffraction (HR-XRPD) was used to assess long-range structure, while Pair Distribution Function (PDF) analysis and Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy provided insights into the local structure. HR-XRPD data revealed that samples with low Zr content (xZr ≤ 0.25) are amorphous. Increasing Zr concentration led to the emergence of a crystalline phase identified as defective fluorite (xZr = 0.375, 0.56). Samples with the highest Zr content (xZr ≥ 0.75) were fully crystalline and exhibited only the fluorite phase. The experimental G(r) functions of the fully crystalline samples in the low r range are suitably fitted by the Weberite structure, mapping the relaxations induced by structural disorder in defective fluorite. These structural insights informed the subsequent EXAFS analysis at the Zr-K and Gd-L₃ edges, confirming the splitting of the cation–cation distances associated with different metal species. Moreover, EXAFS provided a local structural description of the amorphous phases, identifying a consistent Gd-O distance across all compositions. Full article

The nanostructural features of a mechanically alloyed Sb-doped (Ti_0.4Zr_0.6)_0.7Hf_0.3NiSn thermoelectric (TE) Half-Heusler (HH) compound were addressed using Transmission Electron Microscopy (TEM) coupled with Energy Dispersive Spectroscopy measurements and Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy. The EXAFS measurements at the Ni-K, Sn-K, Zr-K, and Hf-L₃-edge were implemented in an effort to reveal the influence of Hf and Zr incorporation into the crystal with respect to their previously measured TE properties. The substitution of Ti by Hf and Zr is expected to yield local lattice distortions due to the different atomic sizes of the dopants or/and electronic charge redistribution amongst the cations. However, the material is characterised by a high degree of crystallinity in both the short and long-range order, on average, and the nominal stoichiometry is identified as (Zr_0.42Hf_0.30Ti_0.28)NiSn_0.98Sb_0.02. The synergistic effect of minimization of extended structural defects or lattice distortions and considerable alloying-induced point defect population contributes to the improved TE properties and leads to the previously reported enhancement of the figure of merit of the mixed HHs. Full article

Owing to global energy demands and climate change resulting from fossil fuel use, technologies capable of converting greenhouse gases into renewable energy resources are needed. One such technology is photocatalytic CO₂ reduction, which utilises solar energy to transform CO₂ into value-added hydrocarbons. However, the application of photocatalytic CO₂ reduction is limited by the inefficiency of existing photocatalysts. In this study, we developed a nitrogen-deficient g-C₃N₄-confined PtCu dual-atom catalyst (PtCu/V_N-C₃N₄) for photocatalytic CO₂ reduction. Aberration-corrected high-angle annular dark-field scanning transmission electron microscopy and X-ray absorption fine structure spectroscopy confirmed the atomic-level anchoring of PtCu pairs onto the nitrogen-vacancy-rich g-C₃N₄ nanosheets. The optimised PtCu/V_N-C₃N₄ exhibited superior photocatalytic performance, with CO and CH₄ evolution rates of 13.3 µmol/g/h and 2.5 µmol/g/h, respectively, under visible-light irradiation. Mechanistic investigations revealed that CO₂ molecules were preferentially adsorbed onto the PtCu dual sites, initiating a stepwise reduction pathway. In situ diffuse reflectance infrared Fourier-transform spectroscopy identified the formation of a key intermediate (HCOO*), whereas interfacial wettability studies demonstrated efficient H₂O adsorption on PtCu sites, providing essential proton sources for CO₂ protonation. Photoelectrochemical characterisation further confirmed the enhanced charge-transfer kinetics in PtCu/V_N-C₃N₄, which were attributed to the synergistic interplay between the nitrogen vacancies and dual-atom sites. Notably, the dual-active-site architecture minimised the competitive adsorption between CO₂ and H₂O molecules, thereby optimising the surface reaction pathways. This study establishes a rational strategy for designing atomically precise dual-atom catalysts through defect engineering, achieving concurrent improvements in activity, selectivity, and charge carrier utilisation for solar-driven CO₂ conversion. Full article

An extensive experimental study of trivalent iron (Fe³⁺) ions in orthorhombic lithium gallate nanocrystals was undertaken. Various spectroscopic methods, such as Raman spectroscopy, extended X-ray absorption fine structure, the Mössbauer effect, electron paramagnetic resonance, photoluminescence, thermoluminescence, and cathodoluminescence were used to investigate the synthesized phosphor. This study revealed the existence of multiple Fe³⁺ sites, out of which the tetrahedral sites are preferentially occupied. Extensive optical studies showed that the Fe³⁺ doped lithium gallate phosphor is a promising candidate for various luminescence and thermoluminescence-related applications in the near-infrared regime. Full article

The urgent need for sustainable CO₂ conversion technologies has driven the development of advanced photocatalysts that harness solar energy. This study employs a CTAB-assisted solvothermal method to fabricate a Z-scheme heterojunction Fe-MOFs/V_O-Bi₂WO₆ (FM/V_O-BWO) for photocatalytic CO₂ reduction. Positron annihilation lifetime spectroscopy (PALS) was employed to confirm the existence of oxygen vacancies, while spherical aberration-corrected transmission electron microscope (STEM) characterization verified the successful construction of heterointerfaces. X-ray absorption fine structure (XAFS) spectra confirmed that the defect configuration and heterostructure changed the surface chemical valence state. The optimized 1.0FM/V_O-BWO composite demonstrated exceptional photocatalytic performance, achieving CO and CH₄ yields of 60.48 and 4.3 μmol/g, respectively, under visible-light 11.8- and 1.5-fold enhancements over pristine Bi₂WO₆. The enhanced performance is attributed to oxygen vacancy-induced active sites facilitating CO₂ adsorption/activation. In situ molecular spectroscopy confirmed the formation of critical CO₂-derived intermediates (COOH* and CHO*) through surface interactions involving four-coordinated and two-coordinated hydrogen-bonded water molecules. Furthermore, the accelerated interfacial charge transfer efficiency mediated by the Z-scheme heterojunction has been conclusively demonstrated. This work establishes a paradigm for defect-mediated heterojunction design, offering a sustainable route for solar fuel production. Full article

Ce₂Pt₆Ga₁₅ is a heavy fermion compound near the quantum critical point (QCP). Its crystal structure may exhibit magnetic frustration due to a honeycomb arrangement; however, stacking faults in the crystal hinder structural analysis. As a local structure probe, extended X-ray absorption fine structure (EXAFS) is less sensitive to stacking faults and is a powerful tool for crystal structure determination. We synthesized single-crystal Ce₂Pt₆Ga₁₅, performed single-crystal and powder X-ray diffraction experiments, and conducted X-ray absorption spectroscopy (XAS) measurements. The composition of Ce₂Pt₆Ga₁₅ deviates from stoichiometry, suggesting Ce and Ga enrichment or Pt site deficiencies. A comparison of X-ray absorption near-edge structure (XANES) at the Ce L₃-edge with reference materials suggests that Ce valence is likely trivalent. To determine the exact structure, we simultaneously analyzed EXAFS spectra at the Ce L₃-, Pt L₃-, and Ga K-edges. The EXAFS spectra of Ce₂Pt₆Ga₁₅ are inconsistent with the hexagonal Sc_0.6Fe₂Si_4.9-type structure but are better explained by an orthorhombic structure with a honeycomb arrangement. Full article